CN103920385A - Oxidation absorption method for converting high-concentration dinitrogen tetroxide waste gas into potassium fertilizer - Google Patents
Oxidation absorption method for converting high-concentration dinitrogen tetroxide waste gas into potassium fertilizer Download PDFInfo
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- CN103920385A CN103920385A CN201410169777.0A CN201410169777A CN103920385A CN 103920385 A CN103920385 A CN 103920385A CN 201410169777 A CN201410169777 A CN 201410169777A CN 103920385 A CN103920385 A CN 103920385A
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- absorption
- waste gas
- nitric acid
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- level
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Links
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 182
- WFPZPJSADLPSON-UHFFFAOYSA-N dinitrogen tetraoxide Chemical compound [O-][N+](=O)[N+]([O-])=O WFPZPJSADLPSON-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000002912 waste gas Substances 0.000 title claims abstract description 41
- 239000003337 fertilizer Substances 0.000 title claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 23
- 230000003647 oxidation Effects 0.000 title claims abstract description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title abstract 4
- 229910052700 potassium Inorganic materials 0.000 title abstract 4
- 239000011591 potassium Substances 0.000 title abstract 4
- 239000007788 liquid Substances 0.000 claims abstract description 131
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 81
- 239000003513 alkali Substances 0.000 claims abstract description 52
- 239000007789 gas Substances 0.000 claims abstract description 46
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000003860 storage Methods 0.000 claims description 44
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 30
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229940072033 potash Drugs 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- 235000015320 potassium carbonate Nutrition 0.000 claims description 14
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 10
- 235000010333 potassium nitrate Nutrition 0.000 claims description 10
- 239000004323 potassium nitrate Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 7
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 claims description 6
- 235000010289 potassium nitrite Nutrition 0.000 claims description 6
- 239000004304 potassium nitrite Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 3
- IRPDISVJRAYFBI-UHFFFAOYSA-N nitric acid;potassium Chemical compound [K].O[N+]([O-])=O IRPDISVJRAYFBI-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 31
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 abstract description 9
- 230000002829 reductive effect Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 238000003915 air pollution Methods 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 210000003739 neck Anatomy 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 41
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000007599 discharging Methods 0.000 description 9
- 230000004907 flux Effects 0.000 description 7
- 238000012856 packing Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- 238000010531 catalytic reduction reaction Methods 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 229910002089 NOx Inorganic materials 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004781 supercooling Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SEPPVOUBHWNCAW-FNORWQNLSA-N (E)-4-oxonon-2-enal Chemical compound CCCCCC(=O)\C=C\C=O SEPPVOUBHWNCAW-FNORWQNLSA-N 0.000 description 1
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- LLBZPESJRQGYMB-UHFFFAOYSA-N 4-one Natural products O1C(C(=O)CC)CC(C)C11C2(C)CCC(C3(C)C(C(C)(CO)C(OC4C(C(O)C(O)C(COC5C(C(O)C(O)CO5)OC5C(C(OC6C(C(O)C(O)C(CO)O6)O)C(O)C(CO)O5)OC5C(C(O)C(O)C(C)O5)O)O4)O)CC3)CC3)=C3C2(C)CC1 LLBZPESJRQGYMB-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- -1 cost is higher Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000009688 liquid atomisation Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Landscapes
- Treating Waste Gases (AREA)
Abstract
The invention relates to an oxidation absorption method for converting high-concentration dinitrogen tetroxide waste gas into potassium fertilizer. The method comprises the following steps of oxidizing and absorbing the dinitrogen tetroixde waste gas with the molar content of 20 to 70 percent collectively through two levels of dilute nitric acid HNO3 and hydrogen peroxide H2O2 to obtain nitric acid, and then converting the nitric acid into potassium fertilizer by utilizing potassium hydroxide KOH alkali liquid. The method can be applied to the working condition that the waste gas pressure, concentration and flow rate are continuously varied, the absorption heat can be radiated in time by adopting large liquid spraying quantity and a kettle liquid cooling method, and a purpose of controlling the temperature can be realized. By adopting the oxidation absorption method, the technical bottle necks of rapidly oxidizing NO, reducing the contents of nitrous acid and nitrite and absorbing and radiating the heat can be broken through. The high-concentration dinitrogen tetroxide waste gas can be absorbed, the emission of toxic acid gas can be reduced, the air pollution can be prevented, and the environmental protection benefit is remarkable. The dinitrogen tetroxide waste gas is converted into the potassium fertilizer, so that waste is changed into treasure, the economic benefit is increased, the processing cost can be offset, and a novel way is provided for processing the tail gas of the nitric acid industry.
Description
Technical field
The present invention relates to a kind of method for processing nitrogen oxide exhaust, specifically a kind of oxidation absorption process that high concentration dinitrogen tetroxide waste gas is converted into potash fertilizer.
Background technology
At space launching site, dinitrogen tetroxide (N
2o
4) liquid in turning filling process, evaporate into the dinitrogen tetroxide (N of gaseous state
2o
4), nitrogen dioxide (NO
2) and nitrogen (N
2) mist, these waste gas need to emit from storage tank and equipment, emission forms hypertoxic tobacco in air, seriously atmosphere pollution, causes very large harm to environment and health of human body.Therefore, need a kind of technology of processing dinitrogen tetroxide waste gas, in time waste gas is converted into eco-friendly material recycling.At present, state, inside and outside the use more widely processing method of nitrous oxides exhaust gas can be divided into dry method and the large class of wet method two, and wherein dry method comprises non-selective catalytic reduction, selective catalytic reduction, SNCR method and absorption method; Wet method comprises absorption process, absorbs reducing process and Absorption via Chemical Complexation etc.Non-selective catalytic reduction H
2, the waste gas such as CO makes NO as reducing agent catalytic reduction
xbe converted into N
2; Selective catalytic reduction NH
3deng reducing agent under metal catalytic, at 300～400 ℃ by NO
xbe reduced to N
2and H
2o; SNCR method with ammonia or urea as reducing agent, reductive NO within the scope of 850 ℃～1100 ℃
xfor N
2method; The absorption such as molecular sieve or active carbon for absorption method; Absorb reducing process for the solution absorption NO such as urea, potassium permanganate, sulphite
x, be converted into HNO
3, N
2, CO
2, MnO
2, Na
2sO
4deng; Absorption process makes water, acid or aqueous slkali absorb NO
x, be converted into HNO
3or nitrate.Because site environment can not be used high temperature process, absorption method is not processed high-concentration waste gas, so dry method is not suitable for the processing of this waste gas.With urea, potassium permanganate, sulfite solution, absorb reductive NO
x, need to consume extra chemicals, cost is higher, and urea absorption produces a large amount of gas, and potassium permanganate and sulfite solution absorb and produce secondary pollution, and water or acid absorb, and tail gas does not reach emission request, and alkali absorbs, and strong carcinogen nitrite concentration is too high.US Patent No. 005637282A has described a kind of method that alkaline hydrogen peroxide solution absorbs low-concentration nitrogen oxide, US Patent No. 006039783A has described a kind of absorption process and equipment that low-concentration nitrogen oxide waste gas is converted into chemical fertilizer, what these patents were processed is low-concentration nitrogen oxide, and product nitrite exceeds standard.
According to the knowledge of the applicant: can be potash fertilizer by the dinitrogen tetroxide exhaust-gas treatment of 60% above high concentration, make nitrogen oxide in tail gas and content of nitrite all reach the absorption techniques of discharging standards, have not been reported.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can adapt to continuous variable working condition high concentration dinitrogen tetroxide waste gas is converted into the oxidation absorption process of potash fertilizer.The method absorption liquid nitrite is less than the discharging standards of 0.5 ppm, and nitrogen oxide in tail gas content is less than 100 mg/m
3discharging standards.
It is as follows that the present invention solves the problems of the technologies described above the technical scheme of taking: a kind of oxidation absorption process that high concentration dinitrogen tetroxide waste gas is converted into potash fertilizer, is characterized in that: by the dinitrogen tetroxide waste gas of molar content 20%～70%, through the rare nitric acid HNO of two-stage
3with hydrogen peroxide H
2o
2co-oxidation absorbs into nitric acid, then is converted into potash fertilizer with potassium hydroxide KOH alkali lye; Concrete grammar is as follows:
Under intermittence and continuous operation mode, by the dinitrogen tetroxide waste gas of molar content 20%～70%, at pressure 0.02～0.2MPa, flow 100～200Nm
3under the condition of/h, enter first grade absorption tower, use the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, be converted into weight percent concentration and be 15%～20% nitric acid; One-level tail gas enters two-level absorption tower, uses the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, and is converted into weight percent concentration and is 15%～20% nitric acid; Secondary tail gas enters three grades of absorption towers again, uses the potassium hydroxide alkali lye that initial weight percent concentration is 16～20% to absorb, by the nitrogen dioxide NO in secondary tail gas
2be converted into potassium nitrate solution KNO
3, micro-nitric oxide NO is converted into potassium nitrite KNO
2; Three grades of tail gas reach discharge standard and pass through high altitude discharge; Each absorption tower absorption liquid flow is 12～13 m
3/ h.
Further, the present invention also comprises: when first grade absorption tower, two-level absorption tower and three grades of absorption towers, when tower reactor absorption liquid temperature reaches 35 ℃, tower reactor absorption liquid is back to corresponding storage tank through return duct, and by the water cooler of installing on return duct, tower reactor absorption liquid is carried out coolingly, be then pumped to respective absorption tower.
Further, potassium nitrate solution, to the pond of being exposed to the sun, is reclaimed to solid nitric acid potassium KNO after moisture evaporation
3chemical fertilizer.
N
2o
4(NO
2) absorption be exothermic reaction, can cause absorption liquid temperature to raise, after temperature surpasses 35 ℃, assimilation effect is very poor, removing reaction heat is another technical problem solved by the invention.By adopting the method for large liquid spray flux and cooling reactor liquid, removed in time and absorbed heat, reach the object of controlling temperature.
The absorption of dinitrogen tetroxide (containing nitrogen dioxide) in water, is a kind of chemical reaction fast, and reaction equation is as (R1)～(R7):
N
2O
4 2NO
2 （R1）
NO
2?+?1/3H
2O?→?2/3HNO
3?+?1/3NO?（R2）
N
2O
4?+?2/3H
2O?→?4/3HNO
3?+?2/3NO?（R3）
NO
2?+?KOH?→?1/2KNO
3?+?1/2KNO
2?+?1/2H
2O?（R4）
N
2O
4?+?2KOH?→?KNO
3?+?KNO
2?+?H
2O?（R5）
NO?+?H
2O
2?→?NO
2?+?H
2O（R6）
HNO
3?+?KOH?→?KNO
3?+?H
2O（R7）
N
2o
4and NO
2can there is equilibrium conversion, so N
2o
4in contain certain NO
2, reaction equation (R1)～(R3) show N
2o
4(NO
2) at H
2absorption in O, has NO to generate, and NO is at H
2solubility in O is very little, easily from absorption liquid, evaporates, and meets air and is partly oxidized to NO
2, causing nitrogen oxide in tail gas concentration over-standard, this is H
2o absorbs NO
xa technical barrier.Reaction equation (R4)～(R5) show N
2o
4(NO
2) can not directly use alkali liquor absorption, otherwise absorption liquid nitrite is very high.The selection of absorbing medium is the key issue that the present invention need to solve.
The absorbing medium of its first grade absorption tower of the present invention and two-level absorption tower is selected HNO
3and H
2o
2mixed solution, be because HNO
3and H
2o
2there is strong oxidation, the nitric oxide NO generating constantly can be oxidized to nitrogen dioxide NO in absorbing
2, by solution, again absorbed, as reaction equation (R6), simultaneously also can be by nitrous acid HNO
2be oxidized to nitric acid HNO
3, by a small amount of potassium nitrite KNO
2be oxidized to potassium nitrate KNO
3, and final absorption liquid only has nitric acid, does not bring other composition into, H
2o
2in absorption, be consumed; Pass through again third level potassium hydroxide KOH alkali liquor absorption, by the nitrogen dioxide NO in secondary tail gas
2be converted into potassium nitrate KNO
3, micro-nitric oxide NO is converted into potassium nitrite KNO
2, reach nitrogen oxide in tail gas NO
xcontent is less than 100 mg/m
3discharging standards, potassium nitrite KNO in absorption liquid
2content is less than the discharging standards of 0.5 ppm.In the salpeter solution producing and potassium hydroxide solution and generate the potassium nitrate solution of percentage by weight 16%～20%, after being exposed to the sun, become solid potash fertilizer, residual H in being exposed to the sun
2o
2can be by a small amount of KNO
2be oxidized to KNO
3and autophage and decomposition.
The present invention combines the method absorbing in conjunction with the absorption of one-level potassium hydroxide alkali lye with hydrogen peroxide acid solution with the rare nitric acid of two-stage, reach the object that high concentration dinitrogen tetroxide is converted into potash fertilizer.Nitrogen oxide is a kind of main atmosphere pollution, must process national standard and could discharge, and high concentration dinitrogen tetroxide exhaust emission is extremely serious, is absorbed processing, has reduced noxious acidic gas discharging, and air conservation has significant environmental benefit.Dinitrogen tetroxide waste gas is converted to potash fertilizer, turns waste into wealth, created economic benefit, offset processing cost, also for nitric acid industry vent gas treatment provides a new approach.
The present invention, in the application of base, Gansu, facts have proved that nitrogen oxide in tail gas concentration and absorption liquid nitrite can reach discharging standards.The present invention can adapt to the operating mode that exhaust gas pressure, concentration and flow constantly change, and by adopting the method for large liquid spray flux and cooling reactor liquid, can remove in time and absorb heat, reaches the object of controlling temperature.The invention solves nitric oxide NO and be oxidized rapidly, reduce nitrous acid and content of nitrite, three technical bottlenecks of absorption heat release.
Use for the equipment of high concentration dinitrogen tetroxide waste gas harmless treatment and realize the present invention.The described device structure for the harmless treatment of high concentration dinitrogen tetroxide waste gas is roughly as follows:
An equipment for the harmless treatment of high concentration dinitrogen tetroxide waste gas, is characterized in that: comprise first grade absorption tower, two-level absorption tower and three grades of absorption towers; Top, absorption tower at different levels is connected with air inlet pipeline and absorption liquid feed tube, the air inlet pipeline of first grade absorption tower connects processed source of the gas, two-level absorption tower air inlet pipeline is connected with first grade absorption tower, three grades of absorption tower air inlet pipelines are connected with two-level absorption tower, the absorption liquid feed tube of one-level, two-level absorption tower connects acid solution storage tank, the absorption liquid feed tube on three grades of absorption towers connects alkali lye storage tank, on each absorption liquid feed tube, liquid pump is installed, bottom, absorption tower at different levels is provided with the tower bottoms return duct being connected with corresponding storage tank, on tower bottoms return duct, water cooler is installed.This equipment and the present invention submit application for a patent for invention on the same day to, and title non-pressure process absorbs the equipment of high concentration nitrogen oxide.
Accompanying drawing explanation
Fig. 1 is the equipment for the harmless treatment of high concentration dinitrogen tetroxide waste gas, is also dinitrogen tetroxide waste gas absorption method flow diagram of the present invention;
Fig. 2 is H
2o
2concentration control flow chart;
Fig. 3 is concentration of lye control flow chart.
In figure: 1-acid solution storage tank, 2-H
2o
2storage tank, 3-one-level absorbs liquid pump, 4-one-level absorption liquid feed tube, 5-one-level absorption liquid electromagnetic flowmeter, 6-one-level absorption liquid control valve, 7-first grade absorption tower, 8-one-level liquid level gauge, 9-one-level still liquid switch valve, 10-one-level tower bottoms recovery tube, 11-N
2o
4waste gas source of the gas, 12-waste gas orifice flowmeter, 13-one-level air inlet adjustment valve, 14-one-level offgas duct, also be two-level absorption tower air inlet pipeline, 15-two-level absorption tower, 16-secondary absorbs liquid pump, 17-secondary absorption liquid feed tube, 18-secondary tower bottoms return duct, 19-secondary offgas duct, also be three grades of absorption tower air inlet pipelines, 20-three grades of absorption towers, 21-alkali lye storage tank, 22-three grades of absorption liquid pumps, 23-three grades of absorption liquid feed tubes, 24-three grades of tower bottoms return ducts, 25-join alkali case, 26-three grades of offgas duct, 27-acid solution discharge line, 28-alkali lye discharge line, 29-one-level water cooler, 30-two-stage water-cooling is device but, 31-three grades of water coolers, 32-H
2o
2pump, 33-liquid distribution pipe, 34-H
2o
2electromagnetic flowmeter, 35-electric switching valve, 36-join alkali circulating pump, 37-low-concentration alkali liquor pipe, 38-high-concentration alkali liquor pipe, 39-pH transmitter.
The specific embodiment
As shown in Figure 1: a kind of equipment for the harmless treatment of high concentration dinitrogen tetroxide waste gas, comprises first grade absorption tower 7, two-level absorption tower 15 and three grades of absorption towers 20; Top, absorption tower at different levels is connected with air inlet pipeline and absorption liquid feed tube; Be that first grade absorption tower 7 tops are provided with one-level air inlet pipeline and one-level absorption liquid feed tube 4, two-level absorption tower 15 tops are provided with one-level offgas duct 14 and 20 tops, 17, three grades of absorption towers of secondary absorption liquid feed tube are provided with secondary offgas duct 19 and the three grades of absorption liquid feed tubes 23 that are connected with two-level absorption tower; One-level air inlet pipeline and processed N
2o
4waste gas source of the gas 11 connects, and two-level absorption tower air inlet pipeline 14 is connected with first grade absorption tower 7, and three grades of absorption tower air inlet pipelines 19 are connected with two-level absorption tower 15; Three grades of absorption towers 20 are provided with 26 outlets of 26, three grades of offgas duct of three grades of offgas duct and are directly communicated with atmosphere.
One-level absorption liquid feed tube 4 is connected 1, three grade of absorption liquid feed tube of acid solution storage tank 23 and connects alkali lye storage tank 21 with secondary absorption liquid feed tube 17; On each absorption liquid feed tube, liquid pump is installed, one-level absorption liquid feed tube 4 is installed one-level absorption liquid pump 3, and secondary absorption liquid feed tube 17 is installed secondarys and absorbed liquid pumps 16, and secondary absorption liquid feed tube 23 is installed three grades of absorption liquid pumps 22; Bottom, absorption tower at different levels is provided with the tower bottoms recovery tube being connected with corresponding storage tank, on tower bottoms recovery tube, water cooler is installed, be that first grade absorption tower 7 bottoms are provided with the one-level tower bottoms recovery tube 10 being connected with acid solution storage tank 1, two-level absorption tower 15 is provided with 18, the three grades of absorption towers 20 of secondary tower bottoms recovery tube that are connected with acid solution storage tank 1 and is provided with three grades of tower bottoms recovery tubes 24 that are connected with alkali lye storage tank 21; On one-level tower bottoms return duct 10, one-level water cooler 29 is installed, two-stage water-cooling is installed on secondary tower bottoms return duct 18 and but on 30, three grades of tower bottoms return ducts 24 of device, three grades of water coolers 31 is installed.
One-level air inlet pipeline is provided with waste gas orifice flowmeter 12 and one-level air inlet adjustment valve 13, is respectively used to observe charge flow rate and regulates charge flow rate; On the liquid outlet end one-level absorption liquid feed tube 4 of one-level absorption liquid pump 3, one-level absorption liquid electromagnetic flowmeter 5 and one-level absorption liquid control valve 6 are installed successively, are respectively used to observe feed liquor flow and regulate feed liquor flow; One-level liquid level gauge 8 is installed in first grade absorption tower 7 bottoms, and one-level still liquid switch valve 9 is installed on one-level tower bottoms return duct 10, and one-level liquid level gauge 8 is electrically connected to one-level still liquid switch valve 9, and when liquid level reaches setting value, one-level still liquid switch valve 9 is opened automatically; Acid solution storage tank 1 is connected with H
2o
2storage tank 2, acid solution discharge line 27 is installed in acid solution storage tank 1 bottom, and alkali lye storage tank 21 is connected with joins alkali case 25, and alkali lye discharge line 25 is installed in alkali lye storage tank 21 bottoms.
High concentration dinitrogen tetroxide waste gas being converted into an oxidation absorption process for potash fertilizer, is under intermittence and continuous operation mode, by the dinitrogen tetroxide waste gas of molar content 20%～70%, at pressure 0.02～0.2MPa, flow 100～200Nm
3under the method condition of/h, enter first grade absorption tower, use the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, be converted into weight percent concentration and be 15%～20% nitric acid; One-level tail gas enters two-level absorption tower, uses the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, and is converted into weight percent concentration and is 15%～20% nitric acid; Secondary tail gas enters three grades of absorption towers again, uses the potassium hydroxide alkali lye that initial weight percent concentration is 16～20% to absorb, by the nitrogen dioxide NO in secondary tail gas
2be converted into potassium nitrate solution KNO
3, micro-nitric oxide NO is converted into potassium nitrite KNO
2; Three grades of tail gas reach discharge standard and pass through high altitude discharge; Each absorption tower absorption liquid flow is 12～13 m
3/ h.The concrete key step of implementing has:
The first, absorption liquid is equipped with
Acid solution storage tank volume 10 m
3, rare nitric acid of preparation 3%～5% and 2% H
2o
2solution is totally 7 m
3; Alkali lye storage tank volume 10 m
3, KOH alkali lye 3 m of preparation 16%～20%
3.
The second, absorption liquid circulation and flow-control
With absorbing liquid pump, absorption liquid is delivered to the tower top feed tube on absorption tower, from liquid distribution trough, is evenly sprayed on filling surface, after packing layer, flow to tower reactor, from tower reactor, enter acid solution or alkali lye storage tank, form circulation.By electromagnetic flowmeter, flow quantity control instrument and electric control valve, controlling absorption liquid flow is 12 ~ 13 m
3/ h.
Three, absorbing tower liquid-level is controlled
With fluid level transmitter, liquid level controller and electric switching valve, control tower reactor liquid level between 600～800mm, to realize fluid-tight, prevent that gas from overflowing from tower reactor.
Four, absorption liquid temperature is controlled
Absorption liquid temperature is controlled and is adopted in two ways, and the one, adopt large liquid spray flux, take away rapidly heat, the 2nd, on the still liquid return line on absorption tower, water cooler is set, to the still liquid of discharging, carry out cooling.
Five, N
2o
4exhaust gas flow is controlled
Open intake valve, allow N
2o
4waste gas enters absorption tower from tower top, and with orifice flowmeter, flow quantity control instrument and control valve, controlling exhaust gas flow is 150 Nm
3/ h.
Six, absorption process
Waste gas is through the rare HNO of two-stage
3and H
2o
2after absorption, most N
2o
4(NO
2) being converted into salpeter solution, a small amount of tail gas enters third level alkali absorption tower and generates KNO
3solution, tail gas enters air by high altitude discharge after reaching discharge standard.
Seven, soda acid absorption liquid neutralization
2/3 sour absorption liquid is pumped into alkali lye storage tank and neutralize, regulate alkali concn, with industrial ph, control and be neutralized to pH=6～8, the potassium nitrate solution of generation is expelled to the outdoor pond of being exposed to the sun, and forms solid nitric acid potassium fertilizer after evaporating moisture.
Eight, emissions concentration detects
On tail gas discharging pipe, establish NOx concentration detector, detection record NOx concentration, detects content of nitrite with rear with chromatography of ions in absorption liquid automatically.
Below in conjunction with Fig. 1, method flow of the present invention is described in further detail.The chemicals percentage below relating to is mass percent concentration.
In acid solution storage tank 1, prepare 3%～5% nitric acid and 2% H
2o
2solution is totally 7 m
3, 30% H
2o
2raw material is contained in storage tank 2, by one-level, absorb liquid pump 3 rare nitric acid absorption liquid is pumped into the tower top of first grade absorption tower 7 from acid solution storage tank 1, absorption liquid is through one-level absorption liquid electromagnetic flowmeter 5 and one-level absorption liquid control valve 6, with FEEDBACK CONTROL adjust flux to 12.5～15 m
3/ h.Rare nitric acid absorption liquid in the mode of jet from first grade absorption tower spray and,
After packing layer, flow into tower reactor, tower reactor has magnetic turnover plate type one-level liquid level gauge 8 and electronic one-level still liquid switch valve 9, controlling tower reactor liquid level is 600～800mm, when still liquid runs up to after 800mm height, one-level still liquid switch valve is opened, and still liquid flows back to acid solution storage tank 1 after supercooling, absorption liquid constantly circulates, until absorb, finishes; The cooling water inlet temperature of one-level water cooler 29 is controlled at below 25 ℃, and flow is 1m
3/ h, after still liquid cooling but, temperature is down to below 30 ℃.
Secondary absorbs liquid pump 16 rare nitric acid absorption liquid 17 is pumped into the top of two-level absorption tower 15 from acid solution storage tank 1, from liquid distribution trough spray and under with pattern, pass through packing layer, flow into tower reactor, still liquid 18 flows back to acid solution storage tank 1 after supercooling, absorption liquid constantly circulates, and finishes two_stage flow and the same one-level of liquid level parameter until absorb, the two-stage water-cooling but cooling water inlet temperature of device 30 is controlled at below 25 ℃, and flow is 1m
3/ h, the cooling rear temperature of still liquid 18 is down to below 30 ℃.
In alkali lye storage tank 21, pack 3m into
3demineralized water, 500 kg solid KOH raw materials are contained in joins in alkali case 25, according to the method for Fig. 3, be mixed with 16%～20% alkali lye, with three grades of absorption liquid pumps 22, will absorb 20 tops, liquid pump to three grade absorption tower, and with spray pattern, pass through after packing layer, tower reactor, still liquid 24 flows back in alkali lye storage tank 21 after supercooling, alkali absorption liquid constantly circulates until absorb end, three grades of liquid levels and the same one-level of flow parameter, the cooling water inlet temperature of three grades of water coolers 31 is controlled at below 25 ℃, and flow is 1 m
3/ h, three grades of cooling rear temperature of tower bottoms are down to below 30 ℃.
Open after three absorption liquid pumps Flow-rate adjustment to 12.5～15 m
3/ h, tower reactor liquid level is controlled at 600～800 mm, and after 15 minutes, packing layer is completely moistening, after flow, level stability, opens electronic one-level air inlet adjustment valve 13.N
2o
4waste gas 11 enters the top of first grade absorption tower 7, adjust flux to 150 Nm through orifice flowmeter 12, one-level air inlet adjustment valve 13
3/ h, gas-liquid contacts at tower top, moves downward, and the impact of gas makes absorption liquid atomization, impels gas-liquid fully to mix.In the process of gas-liquid mixed, there is chemical reaction fast, generate 2/3 HNO
3with 1/3 NO, heat release simultaneously, large liquid spray flux can be defined as away heat, reduces tower top temperature, and low temperature is conducive to absorb.NO is insoluble in water, and because tower top pressure is high, NO can move downward to packing layer along with liquid, and in the process of motion, NO is by H
2o
2and HNO
3oxidation, generates NO
2, again by H
2o absorbs and generates HNO
3oxidation absorbs so repeatedly, to packing layer bottom, gas-liquid enters tower reactor, realizes gas-liquid separation, liquid flows back to acid solution storage tank 1, unabsorbed tail gas enters two-level absorption tower 15 by one-level offgas duct 14, proceeds to be oxidized absorption process, and secondary tail gas is from tower reactor is separated, by secondary offgas duct 19, enter three grades of alkali absorption towers 20, the Main Ingredients and Appearance of secondary tail gas is the NO evaporating
2with a small amount of unabsorbed NO, appellation acid gas, in three grades of alkali absorption towers 20, acid gas is neutralized by KOH, generates KNO
3with a small amount of KNO
2, absorption liquid flows back to 21, three grades of tail gas of alkali lye storage tank and passes through three grades of offgas duct 26 after NOx concentration monitor, and high altitude discharge enters atmosphere.
After absorption finishes, 2/3 acid solution is pumped into alkali lye storage tank 21 from acid solution storage tank 1 and neutralize.
Fig. 2 is H
2o
2preparation process: 30% H
2o
2material liquid is stored in storage tank 2, uses H
2o
2pump 32 is by H
2o
2solution is delivered in acid solution storage tank 1 through liquid distribution pipe 33, H
2o
2the H that flow is installed with liquid distribution pipe 33
2o
2electromagnetic flowmeter 34, electric switching valve 35 and H
2o
2pump 32 is controlled, when integrated flux reaches 0.5m
3after, close H
2o
2pump 32 and electric switching valve 35, now H in acid solution
2o
2concentration is the H in acid solution after 2%, 1h
2o
2be consumed to after 0.1%, again open H
2o
2pump 32 and electric switching valve 35, H
2o
2pumping 0.5 m
3h
2o
2to acid solution storage tank 1, maintain H
2o
2concentration, 0.1%～2%, finishes until absorb.
Alkali liquid compounding flow process is shown in Fig. 3: in alkali lye storage tank 21, pack 3 m into
3demineralized water, 500 kg solid KOHs pack into joins in alkali case 25, with joining alkali circulating pump 36, low-concentration alkali liquor is delivered to and is joined in alkali case 25 through low-concentration alkali liquor pipe 37, high-concentration alkali liquor after dissolved solid KOH is through high-concentration alkali liquor pipe 38, flow back into alkali lye storage tank 21, KOH is dissolved with certain hour, and concentration of lye raises with the continuous dissolving of KOH, finally reaches 16% ~ 20%.
After absorption finishes, 2/3 nitric acid pump in acid solution storage tank 1, to alkali lye storage tank 21, is neutralized to pH=3～4, with pH transmitter 39, detects pH value, then in neutralizer, add appropriate KOH, till making pH=6～8.
After neutralization finishes, potassium nitrate solution pump from alkali lye storage tank 21, to the outdoor pond of being exposed to the sun, is reclaimed to solid K NO after moisture evaporation
3chemical fertilizer.
Case history
By the dinitrogen tetroxide waste gas of molar content 60%, at pressure 0.02～0.2MPa, flow 150Nm
3under the method condition of/h, enter first grade absorption tower, single treatment total amount 450Nm
3, the hydrogenperoxide steam generator co-oxidation that rare nitric acid that use initial weight percent concentration is 3%～5% and initial weight percent concentration are 2% absorbs, absorption liquid volume 7 m
3, one-level tail gas enters two-level absorption tower, and the absorption liquid of two-level absorption tower is identical with the absorption liquid of first grade absorption tower; Secondary tail gas enters three grades of absorption towers again, uses the potassium hydroxide alkali lye that initial weight percent concentration is 16～20% to absorb, alkali absorption liquid volume 3m
3; Absorption liquid flow 12.5～15m
3/ h; Tower reactor liquid level 600～800 mm; Still liquid cooling water flow 1 m
3/ h, 25 ℃ of cooling water inlet temperatures; Soak time 3h; Absorption finishes rear HNO
3concentration 16%, KNO after neutralization
3concentration 16%; In three grades of tail gas, NOx concentration is less than 100 mg/m
3, reach discharge standard and pass through high altitude discharge; KNO in absorption liquid
2content is less than 0.5ppm.
Claims (3)
1. high concentration dinitrogen tetroxide waste gas is converted into an oxidation absorption process for potash fertilizer, it is characterized in that: by the dinitrogen tetroxide waste gas of molar content 20%～70%, through the rare nitric acid HNO of two-stage
3with hydrogen peroxide H
2o
2co-oxidation absorbs into nitric acid, then is converted into potash fertilizer with potassium hydroxide KOH alkali lye; Concrete grammar is as follows:
Under intermittence and continuous operation mode, by the dinitrogen tetroxide waste gas of molar content 20%～70%, at pressure 0.02～0.2MPa, flow 100～200Nm
3under the method condition of/h, enter first grade absorption tower, use the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, be converted into weight percent concentration and be 15%～20% nitric acid; One-level tail gas enters two-level absorption tower, uses the hydrogenperoxide steam generator co-oxidation that rare nitric acid that initial weight percent concentration is 3%～5% and initial weight percent concentration are 0.1%～2% to absorb, and is converted into weight percent concentration and is 15%～20% nitric acid; Secondary tail gas enters three grades of absorption towers again, uses the potassium hydroxide alkali lye that initial weight percent concentration is 16～20% to absorb, by the nitrogen dioxide NO in secondary tail gas
2be converted into potassium nitrate solution KNO
3, micro-nitric oxide NO is converted into potassium nitrite KNO
2; Three grades of tail gas reach discharge standard and pass through high altitude discharge; Each absorption tower absorption liquid flow is 12～13 m
3/ h.
2. a kind of oxidation absorption process that high concentration dinitrogen tetroxide waste gas is converted into potash fertilizer as claimed in claim 1, it is characterized in that: when first grade absorption tower, two-level absorption tower and three grades of absorption towers, when tower reactor absorption liquid temperature reaches 35 ℃, the absorption liquid that is back to corresponding storage tank is carried out cooling with water cooler, its temperature is down to below 30 ℃, is then delivered to respective absorption tower.
3. a kind of oxidation absorption process that high concentration dinitrogen tetroxide waste gas is converted into potash fertilizer as claimed in claim 1 or 2, is characterized in that: potassium nitrate solution, to the pond of being exposed to the sun, is reclaimed to solid nitric acid potassium KNO after moisture evaporation
3chemical fertilizer.
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| CN111185136A (en) * | 2020-01-18 | 2020-05-22 | 中国人民解放军火箭军工程大学 | Dinitrogen tetroxide absorbent, preparation method and application |
| CN112007496A (en) * | 2020-08-25 | 2020-12-01 | 中国人民解放军63921部队 | Method and system for treating dinitrogen tetroxide waste liquid |
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| CN103920385B (en) | 2016-04-06 |
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